Journal of Oleo Science

Copyright 2012 by Japan Oil Chemists Society

J. Oleo Sci. 61, (6) 303-309 (2012)

DSC evaluation of extra virgin olive oil stability

under accelerated oxidative test: effect of fatty acid
composition and phenol contents
Lorenzo Cerretani1, Alessandra Bendini2, Massimiliano Rinaldi3, Maria Paciulli3,
Stefano Vecchio4 and Emma Chiavaro3
1
Dipartimento di Economia e Ingegneria Agrarie, Universit di Bologna, P.zza Goidanich, Cesena (FC), I-47521, Italy
2
Dipartimento di Scienze degli Alimenti, Universit di Bologna, p.zza Goidanich 60, I-47521 Cesena (FC), Italy
3
Dipartimento di Ingegneria Industriale, Universit degli Studi di Parma, Parco Area delle Scienze 181/A, I-43124 Parma, Italy
4
Dipartimento di Scienze di Base e Applicate all'Ingegneria, via del Castro Laurenziano 7, I-00185 Roma, Italy

Abstract: Three extra virgin olive oils having different fatty acid compositions and total phenol contents
were submitted to an accelerated storage test at 60 for up to 21 weeks. Their oxidative status, evaluated
by peroxide values and total phenolic content, was related to differential scanning calorimetry cooling
profiles and thermal properties. Changes in crystallization profiles were consistent starting from 12 weeks
for the two oil samples (B and C) that had a higher content of linoleic acid and medium/low amounts of
phenols, respectively, whereas they became detectable at the end of the test for the remaining oil (sample A).
Decrease of crystallization enthalpy and shift of transition towards lower temperature were also evident at 4
weeks of storage for samples B and C, whereas the same changes in the transition profile were noticeable at
12 weeks for sample A. Differential scanning calorimetry appears to be suitable for the discrimination of
oxidative status of extra virgin olive oils with widely different fatty acid composition.

Key words: Cooling, Differential scanning calorimetry, Extra virgin olive oil, Fatty acids, Total phenols

1 INTRODUCTION Evoo bottles stored at room temperature, which can

Extra virgin olive oilEvoois widely consumed in the
countries of the Mediterranean Area. The presence of high
percentages of oleic acid and minor components with anti-
oxidant activityi.e. tocopherols, phenolic compoundsin
an ideal ratio makes its use very desirable for an increasing
number of the European consumers who value the func-
tional and nutritional values of food1. In this context, a
health claim on the protection of low-density lipoprotein
LDLparticles from oxidative damage by polyphenols in
oliveolive fruit, oil and mill waste waters as Olea euro-
paea L. extract and leafwas recently approvedApril 8th
2011by the EFSA Panel on Dietetic Products, Nutrition
and Allergies2.
Evoo presents a relatively high stability to autoxidation
from 12 to18 months , but this stability differs in rela-
tion with the high variability of its composition, and in par-
ticular to the content of oleic acid55-83and phenolic
3
compounds50 to 1000 mg/kg . In addition, there is little
control of shelf life in many worldwide retail markets for
develop high levels of oxidation leading to undesirable
flavour. Thus, new, simple and fast methods are needed for
the evaluation of oxidative status of Evoo, avoiding expen-
sive and time consuming techniques and assuring correct
classification among legally defined commercial catego-
ries4.
Differential scanning calorimetryDSCis a well known
thermoanalytical technique that is used in several applica-
tions in the field of vegetable oils 5, 6. In recent years,
several publications have emerged on the use of DSC for
the assessment of Evoo quality79. These have studied the
cooling and heating thermal properties and established the
composition of Evoo in terms of triacylglycerols, fatty acids
and minor components10, 11, also using statistical approach-
es12, 13.
DSC was also found to be a valuable tool for assessing
the oxidative deterioration of vegetable oils14. Its applica-
tion to evaluate the degree of thermo-oxidation after con-
ventional heating has been reported for Evoo15as well as

Correspondence to: Emma Chiavaro, Dipartimento di Ingegneria Industriale, Universit degli Studi di Parma, viale Usberti 181/A,
I-43124 Parma, Italy
E-mail: emma.chiavaro@unipr.it
Accepted December 13, 2011 (received for review October 25, 2011)
Journal of Oleo Science ISSN 1345-8957 print / ISSN 1347-3352 online
http://www.jstage.jst.go.jp/browse/jos/http://mc.manusriptcentral.com/jjocs

303
 L. Cerretani, A. Bendini, M. Rinaldi et al.
for different commercial categories of olive oil after micro-
waving16. The capacity of DSC to discriminate among Evoo
samples having different origins and chemical composition
after microwaving was also recently explored17. On the
other hand, DSC application for the evaluation of autoxida-
tion phenomena has not been widely studied. Changes in
selected thermal parameters have been evaluated on Evoo
samples treated by forced light exposition up to 8 weeks18
or after exposure to air bubbles19. Variations in cooling
transition profiles and related thermal properties were also
studied on a Evoo sample in the presence and in the
absence of a phenolic fraction during accelerated storage
treatment carried out at 60 for up to 4 weeks20.
The aim of the present investigation was to evaluate the
application of DSC cooling curves and related thermal
properties for the assessment of the oxidative status of
three Evoo samples chosen for their different fatty acid
composition and total phenol content, and which are rep-
resentative of the Italian oil market. Evoo samples were
subjected to an accelerated storage test at 60, which is
generally considered to be the optimal temperature to
mimic oxidation that develops during normal storage3.
Only the cooling transition was analyzed, as it is well
known that the crystallization of oils is influenced by
chemical composition.
2 EXPERIMENTAL PROCEDURES
2.1 Samples and storage
Three Italian samples of Evoo obtained from olives
handpicked in 2009 and produced using continuous cold
extraction systems were employed: sample A from Emilia
Romagnablend of Leccino, Frantoio, Moraiolo and local
varieties; sample B from Apulia blend of Ogliarola di
Lecce and Cellina di Nard varieties; sample C from
Emilia Romagna blend of Frantoio, Leccino, Pendolino and
Moraiolo varieties. The samples were selected considering
three estimated levels of total phenol content high,
medium and low, respectively .
Each sample was divided in 4 aliquots43.7 mL, 40 g
and kept in the dark at 60 in a thermostatic ovenISCO,
Milan, Italy
for 21 weeks. Each aliquot was stored in an in-
dividual open glass bottle of 250 mLi.d.5 cm; surface
area exposed to air 19.6 cm2 . Bottles were removed from
the oven after 4, 12 and 21 weeks and immediately ana-
lyzed for their chemical composition and DSC thermal
properties.
2.2 Chemical analysis
Fatty acidFAcompositions were determined on fresh
samples22as fatty acid methyl esters by capillary gas chro-
matography GCanalysis after alkaline treatment. The
results were expressed as area normalization in percent
304
J. Oleo Sci. 61, (6) 303-309 (2012)
. FA were expressed according to their degree of un-
saturation as saturatedSFA, monounsaturatedMUFA
and polyunsaturatedPUFAfatty acids. Peroxide value
POV, expressed as mEq O2/kg lipidswas evaluated ac-
cording to the official methods described in annex III of
EEC Regulation 2568/91 23. Total phenol content,ex-
pressed as mg gallic acid/kg oil, was measured using a
spectrophotometric assay as previously reported24. POV
and total phenols were determined on fresh samples and
after 4, 12 and 21 weeks of storage. Three replicates were
analyzed per sample.
2.3 DSC analysis
Samples of oil8-10 mgwere weighed in aluminium
pans, covers were sealed and analyzed with a DSC Q100
TA Instruments, New Castle, DE, USA. Indiummelting
temperature 156.6, H f28.45 J/gand n-dodecane
melting temperature 9.65, H f216.73 J/gwere
used to calibrate the instrument, and an empty pan was
used as reference. Oil samples were equilibrated at 30
for 8 min and then cooled at 80 at a rate of 2/min.
Dry nitrogen was purged in the DSC cell at a flow rate of
50 cm3/min. DSC cooling curves were analyzed with Uni-
versal Analysis SoftwareVersion 3.9A, TA Instrumentsto
obtain enthalpy of crystallizationJ/g, peak temperature
Tp1 and Tp2 for the major and the minor exothermic peaks,
respectively, onset temperatureTon,and offset tem-
peratureToff, of the transitions. The range of transitions
was calculated as the temperature difference between Ton
and Toff. Three replicates were analyzed per sample.
2.4 Statistical analysis
Data were analyzed using SPSS Version 17.0, SPSS Inc.,
Chicago, IL, USAstatistical software. SPSS was used to
perform one-way-analysis of varianceANOVAand Tukey s
honest significance difference post-hoc test at a 95 con-
fidence levelp 0.05to identify differences both among
storage times for each sample and samples at each storage
time.
3 RESULTS AND DISCUSSION
3.1 Chemical analysis
As shown in Table 1 and Fig. 1a, the three Evoo samples
subjected to the accelerated oxidative test were character-
ized by significant differences in terms of fatty acid compo-
sition and phenolic content. In fact, EvooB presented the
lowest content in oleic acid and the highest in palmitic acid
and linoleic acid, and consequently was the poorest in
MUFA category and the richest in SFA and PUFA classes.
On the other hand, EvooA exhibited significantly high per-
centages of MUFA and low of PUFA due to the specific
contents of oleic acid and linoleic acid. EvooC showed a
 DSC evaluation of extra virgin olive accelerated oxidative test

Table 1Main FA percentages and their classes based fatty acid composition between EvooA and EvooB. These
on the unsaturation degree (SFA, saturated; compositional data are completed by the differences in
MUFA, monounsaturated; PUFA, polyun- total phenol composition among the three Evoo samples
saturated) for the Evoo samples storage time 0, Fig. 1a . In fact, this content can be con-
sidered particularly elevated for EvooA 740 mg gallic acid/
FA () EvooA EvooB EvooC kg oil, moderate for EvooB 505 mg gallic acid/kg oiland
B A
Palmitic acid 13.0 15.5 13.1B low261 mg gallic acid/kg oilfor EvooC, showing signifi-
Stearic acid 2.4A 1.8B 2.1A cant differences among samples. The initial POV values 9.2
A C meq O2/kg lipidswere widely below the legal limit for the
Oleic acid 73.7 64.9 71.6B
extra virgin category for all oils showing an unaltered oxi-
Linoleic acid 6.2C 10.0A 8.1B dative status4.
SFA 15.9B 17.7A 15.7B Taking into account the favourable chemical characteris-
MUFA 77.3A 71.7C 75.6B tics of EvooA in terms of the high ratio between oleic acid
PUFA 6.9 C
10.7 A
8.7B and linoleic acid, as well as the considerable phenolic
A, B, C
content25, it could be expected that this sample was the
The same superscript letters within each row are not
most resistant to oxidative changes. In reality, until the end
significantly different (n3, p < 0.05). RSD 2.5
of the 12th week of thermal stress, the increase in POV of
EvooA was very limited and a consistent rise was seen for
both EvooB and EvooC Fig. 1b . Only at the 21th week of
the accelerated storage test EvooA showed a higher value
of peroxide compounds. Thus, EvooA preserved the
highest phenolic content for the entire time of the test,
even if the decrease in these antioxidant compounds was
already significant after 4 weeks, as previously observed20,
as for the other samplesFig. 1b. It can be hypothesized
that EvooA achieved the phase of accumulation of primary
oxidation products later than EvooB and EvooC, as shown
in Fig. 1b, whereas the increase of POV proceeded slowly
for this sample. This was already observed for samples with
analogous FA composition and high phenol content under
similar oxidation conditions26. After 12 weeks of accelerat-
ed storage, EvooB reached a higher amount of peroxide
compounds than EvooC due to its lower oleic/linoleic
ratio27. At week 21, both samples significantly decreased
in POV likely as a consequence of the conversion of the
primary into secondary oxidation products as well as vola-
tile compounds that were responsible for the off flavour of
Evoo during oxidative deterioration27.

3.2 DSC analysis

Fig. 1Changes in phenolic compounds (a) and POV
(b, normalized data) for Evoo samples A, B and
C at different storage times (weeks). Error bars
represent / 1 standard deviation, (n3).
Bars with the same capital letters within each
sample at different storage times were not sig-
nificantly different (p < 0.05).
J. Oleo Sci. 61, (6) 303-309 (2012)
The patterns of crystallization profiles during storage are
shown in Fig. 2a, b and c for EvooA, EvooB and EvooC, re-
spectively. At time 0, all samples showed the classical crys-
tallization profile of Evoo with two exothermic events, a
majorpeak 1, insert a of Fig. 2 peak at lower temperature
and a minorpeak 2, insert a of Fig. 2at higher tempera-
ture regions of the DSC curves, as described in previous
studies8, 9, 12, 28. Changes in crystallization profiles became
evident for oil samples at different storage times. In fact,
none of the samples showed evident modifications at the
first time of storage, in accordance with a previous study
where an Evoo sample was stored up to 4 weeks under the
same conditions20. A small decrease in the height of peak 1
was observed for EvooB and EvooC, however. In addition,
305
 L. Cerretani, A. Bendini, M. Rinaldi et al.

Heat Flow (W/g) the cooling transition did not show marked changes for
0.8
EvooA up to 12 weeks of storage. At 21 weeks, the major
a 21 weeks
cooling peakpeak 1, insert a of Fig. 2shifted towards
0.6 lower temperature and became broader, also enlarging the
range of transition. Similar changes were evident for EvooB
12 weeks
0.4 and EvooC after a shorter time of storage4 weeks, al-
though the shift in peak 1 appeared to be more consistent
4 weeks than EvooAat 12 weeksin both samples. The profile of
0.2
peak 2 was also altered by oxidation as it became less
evident and flattened, especially for EvooC, at the same
0.0
time of storage. Thus, changes in the transition profiles
0 weeks became evident when lipid oxidation noticeably increased,
-0.2
1 2
in accordance with the POV trends shown in Fig. 1b. All
these changes in the DSC crystallization profile have
-0.4 already been observed for Evoo to conventional15or micro-
-100 -80 -60 -40 -20 0 20 40
wave16, 17thermo-oxidation and are related to the formation
0.8 of lipid oxidation products that may weak and/or hinder in-
b 21 weeks termolecular bonding between TAG molecules leading to
0.6 the formation of more irregular crystals as well as to the in-
crease of the oil viscosity15, 29. Crystallization profiles dra-
12 weeks matically changed at the end of storage for EvooB and
0.4
EvooC, as peak 1 disappeared and the profiles of peak 2
doubled showing a shoulder peak at lower temperature at
0.2 4 weeks about 14.9 and 17.2 for EvooB and EvooC, re-
spectivelythan the original peak. These significant modifi-
0.0 cations of the DSC crystallization profiles of Evoo have not
0 weeks been previously reported, and may be attributable to the
-0.2 high content reached by oxidized lipid moleculesboth
primary and secondary lipid oxidation products.
-0.4
Cooling thermal properties obtained for the three Evoo
-100 -80 -60 -40 -20 0 20 40
samples at 0 time and during storage are summarized in
0.8
Table 2. Thermal properties of unheated oils did not show
21 weeks a trend increasing phenols as EvooB, which exhibited mod-
c
erate phenol content and also showed significantly lower
0.6
enthalpy and a larger range of transitionhigher Ton, Tp2
12 weeks and lower Toff and T p1than the other samples. These
0.4
results confirm previous hypotheses about the absence of a
direct role of phenolic compounds in influencing the DSC
0.2 4 weeks crystallization profile, as no significant differences were re-
cently found among cooling thermal properties for a Evoo
0.0 sample in the presence and absence of phenols20. In con-
0 weeks trast, another study11found an effect of variety on cooling
thermal properties such as Ton and Tp1 for Evoo comparing
-0.2
oils before and after partial phenol removal. Otherwise,
higher Ton, Tp1, Tp2 and lower Toff were previously found for
-0.4
-100 -80 -60 -40 -20 0 20 40 Evoo samples with both a high content of palmitic and lin-
oleic acidsas shown by EvooB in Table 1 , and high statis-
Exo Up Temperature (C)
tical correlations were obtained among the thermal proper-
Fig. 2Representative DSC cooling curves of Evoo ties and amounts of these compounds12.
samples A (a), B (b) and C (c) at different stor- All samples showed a significant decrease in enthalpy of
age times (weeks). crystallization during storage, which became consistent at
different storage times for EvooA 12 weeksin comparison
with EvooB and EvooC4 weeks. A significant shift in
transition towards lower temperature was also observed
306
J. Oleo Sci. 61, (6) 303-309 (2012)
 DSC evaluation of extra virgin olive accelerated oxidative test

Table 2DSC thermal properties obtained from the cooling thermograms of Evoo samples at
different storage times
Storage Enthalpy of
time crystallization Ton () Toff () Range() Tp1 () Tp2 ()
(weeks) (J/g)
Evoo A
0 57.9a A 11.2b A 44.7a A 33.5c D 38.3a A 15.4b A
4 56.1A 11.7A B 46.0B 34.1C 38.5A 15.4A
12 55.2A 11.7A B 46.9C 35.2B 39.0B 15.1A
21 36.4B 12.1C 68.9D 56.7A 60.7C 16.5B
Evoo B
0 56.1a A 10.3a B 48.7c A 38.4a C 42.3b A 12.8a A
4 52.4B 10.6B 50.6B 40.1B 43.2B 12.9A
C B cC A C
12 36.2 10.5 74.0 63.5 67.0 13.7AB
21 n.d. 8.8A n.d. n.d. n.d. 14.9B
Evoo C
0 57.2a A 11.1b C 46.5b A 35.4b B 39.4a A 14.9b A
B C B B B
4 53.0 12.0 47.7 35.7 40.2 15.2A
12 31.6C 12.2B 73.1C 62.0A 66.7C 16.5AB
21 n.d. 9.3b A n.d. n.d. n.d. 17.1B
a, b, c
The same superscript letters within samples at 0 storage time are not significantly different
A, B, C
The same superscript letters within each sample at different storage times are not significantly
different (n3, p < 0.05). n.d.not determined. RSD 2.

for EvooA as Ton and Toff, and both exothermic peaks signifi-
cantly shifted towards lower temperatures enlarging the
range of crystallization in this sample. All these changes
may be related to the formation of lipid oxidation products
that could form mixed and disordered triglyceride crystals.
These crystals require lower energy to crystallize, and also
retard the phase transition30. All these phenomena were
also evident for EvooB and EvooC with the exception of
Ton, which shifted towards higher temperature at the end
of storage. The shift of transition towards higher tempera-
ture has been previously attributed to the increase in diac-
ylglycerol content in Evoo as consequence of lipid hydroly-
sis due to auto 28- or thermo-oxidation phenomena 16,
although a statistical correlation was not found in fresh oil
samples where diacylglycerol amounts were low12. In addi-
tion, EvooB and EvooC did not show marked changes in
thermal property either for trend of changes or their
extent, although oxidative deterioration of EvooB ap-
peared to be more consistent than EvooC at 12 weeks of
storageFig. 1b , in accordance with its fatty acid composi-
tion. In a previous study carried out on microwave thermo-
oxidized Evoo samples, modifications in thermal properties
exhibited a different trend among oils, but the relationship
of these changes with chemical composition and/or oxida-
tion extent was not clearly established as several factors
J. Oleo Sci. 61, (6) 303-309 (2012)
appeared to be involved17. Thus, the relation among Evoo
cooling thermal properties and stability indices, not only
from primary but also from higher oxidation stagesi.e.
secondary and tertiary, should be further investigated by
evaluation of statistical correlations on a large set of oil
samples taking into account both auto- and thermo-oxida-
tion since the lipid kinetics of these phenomena are differ-
ent.
4 CONCLUSIONS
The application of DSC appears to be suitable for the
evaluation of qualitative changes in extra virgin olive under
temperature conditions that best mimic the kinetics of oxi-
dation developing during storage at room temperature.
This could be of interest for producers and traders of this
high quality vegetable oil, since DSC has undisputable ad-
vantages over classical analytical methods as it does not
require sample preparation or solvent utilization, has a
reduced environmental impact and avoids the use of time-
consuming procedures.
Some thermal properties like onset and offset tempera-
tures of crystallization as well as DSC peak temperatures
represent an useful tool for the evaluation of degradation
307
 L. Cerretani, A. Bendini, M. Rinaldi et al.

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